Preparation method of II-VI family water-soluble selenide semiconductor quantum dots

A water-soluble, quantum dot technology, used in chemical instruments and methods, luminescent materials, etc., can solve the problems of affecting fluorescence quantum efficiency, many impurities in quantum dots, and long preparation time, and achieve high fluorescence yield, uniform dispersion, and operation. simple effect

Inactive Publication Date: 2011-08-31
EAST CHINA NORMAL UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

At present, the method for synthesizing quantum dots of selenide in group II-VI compounds in aqueous phase is to synthesize NaHSe or selenite directly react with cadmium source, and grow under reflux at about 100°C and one atmospheric pressure. The degree of dispersion and the fluorescence quantum yield have a certain influence, and the reaction time is long
[0004] The method of the invention overcomes the defects that the quantum dots prepared in the prior art contain more impurities, the energy levels of more impurities affect the fluorescence quantum efficiency, and the preparation time is long, and provides a II-VI water-soluble selenide The preparation method of semiconductor quantum dots has the beneficial effects of high purity, short preparation time and good fluorescence performance

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  • Preparation method of II-VI family water-soluble selenide semiconductor quantum dots
  • Preparation method of II-VI family water-soluble selenide semiconductor quantum dots
  • Preparation method of II-VI family water-soluble selenide semiconductor quantum dots

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Embodiment 1

[0029] 1. Add 0.48 mmol Cd(Ac) 2 2H 2 O was dissolved in 96ml of water, 1.2mmol of mercaptopropionic acid was added, and the pH value was adjusted to about 9.5 with 1mol / L NaOH under stirring, and the solution was transferred to an appropriate three-necked bottle.

[0030]2. Add 0.63 mmol of selenium powder and 1.26 mmol of sodium borohydride and 40 ml of deionized water into a container that has been deoxygenated with nitrogen for a period of time, and react with magnetic stirring at 0°C for 3 hours to obtain a colorless and transparent solution with white boric acid Sodium was precipitated and nitrogen protection was maintained throughout the reaction.

[0031] 3. Take 2ml of sodium borohydride solution and place it in an ice bath. When the temperature drops to 0°C, add a certain amount of 0.51mol / L sulfuric acid solution to the sodium selenium hydride solution drop by drop, and the sulfuric acid and sodium selenium hydride will immediately have a violent reaction. The rea...

Embodiment 2

[0038] 1. Add 0.48 mmol ZnCl 2 Dissolve in 96ml of water, add 1.2 mmol of mercaptoacetic acid, adjust the pH to about 9.5 with 1 mol / L NaOH under stirring, and transfer the solution to a suitable three-necked bottle.

[0039] 2. Configure 0.02M Na 2 Se solution, always under nitrogen protection during the configuration process.

[0040] 3. Take 3mlNa 2 The Se solution is placed in an ice bath. When the temperature drops to 0°C, a certain amount of 0.51mol / L sulfuric acid solution is added dropwise to the solution. The sulfuric acid and sodium selenide react violently immediately, and the selenide is formed. hydrogen gas.

[0041] 4. Under the protection of nitrogen, pass the hydrogen selenide gas directly into the container containing the mixed solution of zinc chloride and thioglycolic acid with the nitrogen. The reaction temperature is 90°C, and the solution immediately changes from colorless to light yellow. This solution is the precursor solution, and the precursor sol...

Embodiment 3

[0044] 1. Add 0.48 mmol HgSO 4 Dissolve in 96ml of water, add 1.5 mmol of mercaptoethylamine, adjust the pH value to about 9.5 with 1 mol / L NaOH under stirring, and transfer the solution to an appropriate three-necked bottle.

[0045] 2. Configure 0.02M Al 2 Se 3 solution, always under nitrogen protection during the preparation process.

[0046] 3. Take 5ml 0.02M Al 2 Se 3 The solution is placed in an ice bath. When the temperature drops to 0°C, a certain amount of 0.51mol / L sulfuric acid solution is added dropwise to the solution. The sulfuric acid and aluminum selenide react violently immediately to produce hydrogen selenide. gas.

[0047] 4. Under the protection of nitrogen, the hydrogen selenide gas is directly passed into the container containing the mixed solution of cadmium nitrate and mercaptoethylamine along with the nitrogen gas. The reaction temperature is 70 ° C. The solution immediately changes from the original colorless to light yellow. This solution is th...

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Abstract

The invention provides a preparation method of II-VI family water-soluble selenide semiconductor quantum dots, which comprises the following specific steps: adding a stabilizer into solution containing soluble cadmium salt, soluble zinc salt or soluble mercury salt, then regulating the pH value of the solution to be be alkaline, then introducing hydrogen selenide gas under inert atmosphere, and reacting till the solution is pale yellow and transparent, thereby preparing solution of a precursor, wherein the molar ratio of the soluble cadmium salt, the soluble zinc salt or the soluble mercury salt to the stabilizer is 1: 3-1: 2. High-temperature and high-pressure fast growth is performed on the solution of the precursor, thereby preparing the II-VI family water-soluble selenide semiconductor quantum dots. For the preparation method, the operation is simple, the cost is low, the toxicity is small, and the prepared II-VI family water-soluble selenide semiconductor quantum dots can be directly used for biological fluorescent marking, clinical diagnosis and other experiments.

Description

technical field [0001] The invention relates to the field of semiconductor material preparation, in particular to a method for preparing II-VI group water-soluble selenide semiconductor quantum dots. Background technique [0002] With the development of material preparation technology, people can make some semiconductor materials into nanocrystalline grains. If the size is smaller than or reaches its excitonic Bohr radius, it is called the quantum dot of the semiconductor material. Due to the quantum size effect, small size effect and surface effect of quantum dots, the physical and chemical properties of raw materials are changed, such as light, magnetism, electricity, force, etc., and the change of their optical properties is widely used. CdSe, ZnSe, Cd(Zn)S, Cd(Zn)Se, Cd(Zn)Te and other II-VI compound semiconductor quantum dots have special fluorescence emission characteristics, which are different from fluorescent organic dyes and have high fluorescence intensity. The f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/88C09K11/89
Inventor 杨琴唐政孙放
Owner EAST CHINA NORMAL UNIV
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